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Acta Cryst. (2004). C60, m69-m72
https://doi.org/10.1107/S0108270103029500
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Bis(2,2'-bi­pyridine-[kappa]2N,N')(1,10-phen­anthroline-[kappa]2N,N')­ruthenium(II) tetra­cyano­platinate(II)

K. Sakai and Y. Miyabe
In the title compound, [Ru(C10H8N2)2(C12H8N2)][Pt(CN)4], cations and anions alternate along the a axis to afford a one-dimensional network. The one-dimensional character arises from the [pi]-[pi] stacking as well as from the electrostatic interactions formed between the phen (1,10-phenanthroline) and [Pt(CN)4]2- units. Two adjacent one-dimensional chains form further stacks based on the [pi]-[pi] stacking interactions between the phen moieties, where the interplanar spacing is 3.50 (1) Å.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103029500/ob1157sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270103029500/ob1157Isup2.hkl
Contains datablock I

CCDC reference: 233111

Comment top

Homogeneous catalysis of platinum(II) complexes in photochemical H2 production from water have been examined in our laboratory by utilizing a well known photosystem consisting of [Ru(bpy)3]2+ (bpy is 2,2'-bipyridine) and methylviologen (usually N,N'-dimethyl-4,4'-bipyridinium dichloride; Sakai & Matsumoto, 1990; Sakai et al., 1993). In this context, we began five years ago to explore the chemistry of double salts consisting of [Ru(bpy)3]2+ derivatives and platinum complexes. Our aim has been to develop water-insoluble crystals involving both the photosensitizing and the H2-evolving centers. Visible-light-induced water splitting into H2 and 0.5O2 might be promoted under dispersion in aqueous media of such hybrid crystals, including their doped systems. As part of these studies, we report here the crystal structure of the title compound, [Ru(bpy)2(phen)][Pt(CN)4], (I) (phen is 1,10-phenanthroline).

The asymmetric unit of (I) consists of an [Ru(bpy)2(phen)]2+ cation and a [Pt(CN)4]2− anion (Fig. 1). The phen ligand of the cation is disordered over two sites. For simplicity, only the structure containing the major phen component, which has an occupancy of 75.2 (5)%, will be discussed below. The cations and anions stack along the a axis in an alternating fashion (Fig. 2). This can be viewed as related to the so-called Magnus green salt, [Pt(NH3)4][PtCl4] (Atoji et al., 1957). The phen unit, having an aromatic system that is slightly larger than the bpy unit, seems to play an important role in stabilizing the one-dimensional network in (I). Thus a more appropriate description is that the phen and [Pt(CN)4]2− units alternate along the a axis (see Figs. 2–4). As shown in Fig. 3, the phen and tetracyanoplatinate planes are not coplanar and are inclined by 21.9 (2)° to one another. The observed short contacts are listed in Table 2. On the other hand, two adjacent chains are stacked as a result of the π–π associations achieved between the phen units. As shown in Fig. 4, two neighbouring phen units form a π–π stack through an inversion center. From the average shift of atoms C6i and C9i [symmetry code: (i) 1 − x, 1 − y, −z] from the mean plane of the phen molecule defined by N1/N2/C1–C12, the interplanar separation is estimated as 3.50 (1) Å. Some relevant C—C contacts are also given in Table 2.

Because the electrostatic and π–π attractive forces are enhanced in the crystal structure of (I), the PtII ion shows a relatively large distortion towards a tetrahedral geometry, in which the Pt1/C33/C36 and Pt1/C34/C35 planes are inclined at an angle of 7.2 (3)°. The selected distances and angles around the coordination geometries in (I) are listed in Table 1.

As recently reported by Sakai, Uchida et al. (2004), it has been ascertained in our laboratory that double salts consisting of [Ru(bpy)3]2+ (which may be classified as a homo-ligand system) tend to give two-dimensional cationic/porous layers in the crystal structure, two-dimensional {[Ru(bpy)3]}n2n+. For instance, the crystal structures of [MII(bpy)3][Pt(oxalato)2] (MII = Ni, Fe and Ru) have been ascertained to comprise very similar two-dimensional cationic/porous layers in which the pores are occupied by the [Pt(oxalato)2]2− anions (unpublished results), even though the structure determination of the tetracyanoplatinate derivatives have been unsuccessful thus far because of the difficulty of crystallizing the materials. At the moment, we think that the one-dimensionality achieved in the crystal structure of (I) is relevant to the lower symmetry in the present mixed-ligand system.

Experimental top

K2[Pt(CN)4]·3H2O (Kojima Chemicals Co. Ltd) was used as received. cis-RuCl2(bpy)2·2H2O was prepared as described previously (Sullivan et al., 1978). [Ru(bpy)2(phen)]Cl2 was previously reported as a trihydrate salt (Baggott et al., 1983) but was prepared as a heptahydrate salt, [Ru(bpy)2(phen)]Cl2·7H2O, by the following method. A mixture of cis-RuCl2(bpy)2·2H2O (0.26 g, 0.5 mmol) and phen (0.099 g, 0.55 mmol) in ethanol (25 ml) was refluxed overnight. After the solution was filtered for the removal of insoluble materials, the filtrate was evaporated to a total volume of 5–10 ml. The solution was added gradually to diethylether (80 ml) with stirring. The orange precipitate deposited was collected by suction filtration and air dried (yield 80%). The compound was recrystallized from hot water before use. Analysis calculated for RuCl2O7N6C32H38: C 48.61, H 4.84, N 10.63%; found: C 48.58, H 4.67, N 10.65%. Diffraction-quality single crystals of (I) were prepared as follows, based on our unique diffusion method as reported for [Pt(bpy)(2-aminopyridine)2][Pt(oxalato)2].2H2O (Sakai et al., 2003) and [Pt(bpy)(2-aminopyridine)2][Pt(CN)4].2H2O (Sakai, Mizota et al., 2004). A petri dish, having a diameter of ca 60 mm and a depth of ca 15 mm, was separated into three zones using filter papers; the central zone (zone 2) must be sandwiched by the other two zones (zones 1 and 3). Zones 1 and 2 (or zones 2 and 3) should be separated by two or three pieces of filter paper, while contact between zones 1 and 3 should be avoided. Water (6 ml) was added to the petri dish, filling all three zones. Finally, solutions of K2[Pt(CN)4]·3H2O (0.015 mmol) in water (1.5 ml) and of [Ru(bpy)2(phen)]Cl2·7H2O (0.015 mmol) in water (1.5 ml) were added dropwise, simultaneously, to zones 1 and 3, respectively. The solution was left to stand at 293 K for a few days. The major product deposited, in the form of orange crystals, was found to be unstable in air, since the crystals rapidly lose water to give an amorphous material on exposure to air at room temperature. The elemental analysis showed that the major product is a pentahydrated salt. Analysis calculated for PtRuO5N10C36H34: C 43.99, H 3.49, N 14.25%; found: C 43.91, H 3.40, N 14.36%. On the other hand, the title compound, (I), which deposited as red prisms as the minor product, was found to be very stable, since it is an anhydrous salt as determined in the present X-ray study. Since the product yield was quite low, the elemental analysis of (I) could not be carried out. There is a possibility that (I) might be contaminated with [Ru(bpy)3]2+, since the disorder phenomena observed around the phen moiety might also be elucidated with a model in which the [Ru(bpy)2(phen)]2+ cations are partly replaced by the [Ru(bpy)3]2+ cations. However, such a possibility can be ruled out because the purity of [Ru(bpy)2(phen)]Cl2·7H2O as well as cis-RuCl2(bpy)2·2H2O has always been carefully checked by 1H NMR in our laboratory. Consequently, the model described below has been judged to be valid.

Refinement top

The 5- and 6-positions of the phen C atoms were found to be disordered over two sites (C5A/C6A and C5B/C6B). In other words, the phen ligand and one of the bpy ligands (involving atoms N5 and N6) are partly replaced by one another. The validy of this model has been checked by examination of the difference Fourier maps generated by PLATON (Spek, 2003). The occupancies of sites A and B converged at 75.2 (5) and 24.8 (5)%, respectively. The anisotropic displacement parameters of atoms C4, C5A, C6A and C7 were very weakly restrained to have similar values. The displacement parameters of atoms C26, C5B, C6B and C29 were also weakly restrained to have similar values. All H atoms, except for those attached to the disordered bpy units, were placed at idealized positions [C—H(bpy) = 0.93 Å], and included in the refinement in a riding-motion approximation, with Uiso(H) values equal to 1.2Ueq(C). H atoms attached to the 3- and 3'-positions of the disordered bpy units were not located. The highest peak was 0.95 Å from atom Pt1, while the deepest hole was 0.85 Å from atom Ru1.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: KENX (Sakai, 2002); software used to prepare material for publication: SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX and ORTEP (Johnson, 1976).

Figures top
[Figure 1] Fig. 1. The structure of (I), showing the atom-labeling scheme. Displacement ellipsoids are shown at the 50% probability level. There is positional disorder of the phen ligand. The site occupation factors of atoms C5A and C6A, and C5B and C6B, are 75.2 (5) and 24.8 (5)%, respectively.
[Figure 2] Fig. 2. The crystal packing of (I), viewed along the b axis, showing two adjacent one-dimensional chains. Atoms C5B and C6B and the H atoms have been omitted for clarity.
[Figure 3] Fig. 3. A view of (I), parallel to the phen plane including atoms C5A and C6A, showing how the [Pt(CN)4]2− anions and the major phen units stack along the a axis. Atoms C5B and C6B and the H atoms have been omitted for clarity.
[Figure 4] Fig. 4. A view of (I), perpendicular to the phen plane including atoms C5A and C6A, showing how the [Pt(CN)4]2− anions and the major phen units stack along the a axis. Atoms C5B and C6B and the H atoms have been omitted for clarity.
Bis(2,2'-bipyridine-κ2N,N')(1,10-phenanthroline-κ2N,N')ruthenium(II) tetracyanoplatinate(II) top
Crystal data top
[Ru(C10H8N2)2(C12H8N2)][Pt(CN)4]Z = 2
Mr = 892.81F(000) = 864
Triclinic, P1? # Insert any comments here.
Hall symbol: -P 1Dx = 1.842 Mg m−3
a = 8.6251 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.7842 (15) ÅCell parameters from 5196 reflections
c = 14.7039 (17) Åθ = 2.7–27.2°
α = 94.557 (2)°µ = 4.85 mm−1
β = 94.063 (2)°T = 296 K
γ = 92.637 (2)°Prism, red
V = 1610.0 (3) Å30.38 × 0.22 × 0.2 mm
Data collection top
Bruker SMART APEX CCD-detector
diffractometer		5785 independent reflections
Radiation source: fine-focus sealed tube4934 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
Detector resolution: 8.366 pixels mm-1θmax = 25.4°, θmin = 2.2°
ω scansh = −10→10
Absorption correction: gaussian
(XPREP in SAINT; Bruker, 2001)		k = −14→15
Tmin = 0.262, Tmax = 0.512l = −17→8
8622 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.068H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.03P)2]
where P = (Fo2 + 2Fc2)/3
5785 reflections(Δ/σ)max = 0.001
452 parametersΔρmax = 0.88 e Å−3
36 restraintsΔρmin = −0.44 e Å−3
Crystal data top
[Ru(C10H8N2)2(C12H8N2)][Pt(CN)4]γ = 92.637 (2)°
Mr = 892.81V = 1610.0 (3) Å3
Triclinic, P1Z = 2
a = 8.6251 (10) ÅMo Kα radiation
b = 12.7842 (15) ŵ = 4.85 mm−1
c = 14.7039 (17) ÅT = 296 K
α = 94.557 (2)°0.38 × 0.22 × 0.2 mm
β = 94.063 (2)°
Data collection top
Bruker SMART APEX CCD-detector
diffractometer		5785 independent reflections
Absorption correction: gaussian
(XPREP in SAINT; Bruker, 2001)		4934 reflections with I > 2σ(I)
Tmin = 0.262, Tmax = 0.512Rint = 0.037
8622 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03036 restraints
wR(F2) = 0.068H-atom parameters constrained
S = 1.00Δρmax = 0.88 e Å−3
5785 reflectionsΔρmin = −0.44 e Å−3
452 parameters
Special details top

Experimental. The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Mean-plane data from final SHELXL refinement run:-

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

-7.2993 (0.0092) x + 3.5561 (0.0262) y + 7.5456 (0.0261) z = 2.8472 (0.0079)

* 0.0867 (0.0026) C33 * −0.0869 (0.0026) C34 * 0.0870 (0.0026) C35 * −0.0868 (0.0026) C36 − 0.0073 (0.0025) Pt1 0.1638 (0.0104) N7 − 0.1651 (0.0092) N8 0.2327 (0.0094) N9 − 0.2042 (0.0083) N10

Rms deviation of fitted atoms = 0.0868

7.6444 (0.0027) x + 1.2344 (0.0153) y − 7.5546 (0.0088) z = 2.6970 (0.0092)

Angle to previous plane (with approximate e.s.d.) = 21.94 (0.15)

* 0.0227 (0.0033) N1 * 0.0034 (0.0032) N2 * −0.0328 (0.0039) C1 * −0.0342 (0.0046) C2 * 0.0111 (0.0050) C3 * 0.0243 (0.0049) C4 * 0.0193 (0.0061) C5A * −0.0124 (0.0067) C6A * −0.0087 (0.0051) C7 * −0.0312 (0.0051) C8 * −0.0101 (0.0046) C9 * 0.0221 (0.0037) C10 * 0.0028 (0.0039) C11 * 0.0238 (0.0040) C12 − 3.6289 (0.0059) N8 − 3.4441 (0.0061) N9 3.4973 (0.0091) C6A_$2 3.4936 (0.0064) C7_$2 3.5161 (0.0069) C8_$2 3.4950 (0.0065) C9_$2 3.1209 (0.0072) C36_$3 3.3610 (0.0045) Pt1_$3

Rms deviation of fitted atoms = 0.0211

3.5694 (0.0129) x + 5.0530 (0.0210) y + 10.9090 (0.0167) z = 8.4383 (0.0147)

Angle to previous plane (with approximate e.s.d.) = 86.25 (0.09)

* 0.0055 (0.0026) N3 * 0.0056 (0.0030) C13 * −0.0105 (0.0033) C14 * 0.0049 (0.0035) C15 * 0.0059 (0.0034) C16 * −0.0113 (0.0029) C17

Rms deviation of fitted atoms = 0.0077

2.3454 (0.0160) x + 5.7016 (0.0209) y + 11.5204 (0.0173) z = 8.3869 (0.0170)

Angle to previous plane (with approximate e.s.d.) = 8.76 (0.26)

* 0.0073 (0.0028) N4 * −0.0105 (0.0032) C18 * 0.0058 (0.0036) C19 * 0.0020 (0.0040) C20 * −0.0052 (0.0037) C21 * 0.0006 (0.0031) C22

Rms deviation of fitted atoms = 0.0062

−2.9436 (0.0171) x + 11.6426 (0.0104) y − 4.8901 (0.0282) z = 5.9982 (0.0228)

Angle to previous plane (with approximate e.s.d.) = 85.53 (0.14)

* −0.0174 (0.0031) N5 * 0.0185 (0.0035) C23 * −0.0010 (0.0040) C24 * −0.0169 (0.0042) C25 * 0.0175 (0.0038) C26 * −0.0006 (0.0032) C27

Rms deviation of fitted atoms = 0.0144

−3.5040 (0.0160) x + 10.4438 (0.0162) y − 7.0274 (0.0269) z = 3.9492 (0.0215)

Angle to previous plane (with approximate e.s.d.) = 11.31 (1/4)

* 0.0201 (0.0030) N6 * −0.0295 (0.0032) C28 * 0.0117 (0.0039) C29 * 0.0144 (0.0044) C30 * −0.0233 (0.0041) C31 * 0.0066 (0.0036) C32

Rms deviation of fitted atoms = 0.0192

−7.5259 (0.0071) x + 3.9320 (0.0255) y + 6.5557 (0.0194) z = 2.7142 (0.0056)

Angle to previous plane (with approximate e.s.d.) = 67.21 (0.15)

* −0.0073 (0.0022) Pt1 * −0.0112 (0.0052) C33 * 0.0308 (0.0039) C36 * 0.0071 (0.0033) N7 * −0.0194 (0.0025) N10

Rms deviation of fitted atoms = 0.0176

−7.0988 (0.0084) x + 2.8444 (0.0227) y + 8.4824 (0.0183) z = 2.8636 (0.0085)

Angle to previous plane (with approximate e.s.d.) = 9.22 (1/5)

* 0.0087 (0.0021) Pt1 * 0.0168 (0.0044) C34 * −0.0400 (0.0045) C35 * −0.0109 (0.0028) N8 * 0.0254 (0.0029) N9

Rms deviation of fitted atoms = 0.0233

−7.4468 (0.0110) x + 3.9783 (0.0366) y + 6.7821 (0.0351) z = 2.7718 (0.0097)

Angle to previous plane (with approximate e.s.d.) = 8.45 (0.28)

* 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) C33 * 0.0000 (0.0000) C36

Rms deviation of fitted atoms = 0.0000

−7.1204 (0.0130) x + 3.1236 (0.0336) y + 8.2847 (0.0332) z = 2.8991 (0.0097)

Angle to previous plane (with approximate e.s.d.) = 7.18 (0.34)

* 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) C34 * 0.0000 (0.0000) C35

Rms deviation of fitted atoms = 0.0000

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pt1−0.01509 (2)0.263187 (14)0.237732 (12)0.05383 (8)
Ru10.49553 (4)0.73465 (3)0.26766 (2)0.04449 (10)
N10.5673 (4)0.5934 (3)0.3110 (2)0.0472 (8)
N20.4075 (4)0.6336 (3)0.1584 (2)0.0479 (9)
N30.6816 (4)0.7719 (3)0.1935 (2)0.0489 (8)
N40.4261 (4)0.8684 (3)0.2121 (2)0.0509 (9)
N50.5737 (5)0.8215 (3)0.3875 (2)0.0584 (10)
N60.3094 (4)0.7163 (3)0.3455 (2)0.0517 (9)
N7−0.0538 (8)0.0495 (5)0.3237 (4)0.119 (2)
N80.2184 (6)0.3504 (5)0.4016 (3)0.110 (2)
N9−0.0095 (6)0.4879 (4)0.1690 (3)0.0955 (16)
N10−0.2159 (6)0.1695 (4)0.0615 (3)0.0794 (13)
C10.6417 (5)0.5749 (4)0.3906 (3)0.0585 (12)
H10.67000.63110.43360.070*
C20.6773 (6)0.4752 (4)0.4106 (4)0.0758 (15)
H20.72990.46520.46640.091*
C30.6368 (6)0.3908 (4)0.3497 (4)0.0795 (16)
H30.66360.32380.36310.095*
C40.5547 (6)0.4060 (4)0.2674 (4)0.0684 (13)
C5A0.5000 (8)0.3278 (5)0.2000 (5)0.077 (2)0.752 (5)
H50.52140.25830.20780.092*0.752 (5)
C5B0.425 (3)0.8817 (18)0.5896 (16)0.082 (6)0.248 (5)
H5B0.44680.91970.64600.099*0.248 (5)
C6A0.4162 (10)0.3506 (6)0.1230 (5)0.084 (2)0.752 (5)
H60.38020.29500.08100.101*0.752 (5)
C6B0.270 (3)0.8315 (19)0.5648 (16)0.095 (6)0.248 (5)
H6B0.20310.83980.61140.114*0.248 (5)
C70.3809 (6)0.4506 (4)0.1032 (3)0.0696 (14)
C80.2968 (7)0.4786 (5)0.0256 (3)0.0823 (16)
H80.25710.4268−0.01900.099*
C90.2721 (6)0.5800 (5)0.0144 (3)0.0736 (15)
H90.21650.5985−0.03790.088*
C100.3304 (5)0.6569 (4)0.0817 (3)0.0555 (12)
H100.31500.72700.07290.067*
C110.4338 (5)0.5314 (3)0.1684 (3)0.0502 (10)
C120.5211 (5)0.5088 (3)0.2503 (3)0.0510 (11)
C130.8036 (5)0.7114 (4)0.1816 (3)0.0586 (12)
H130.80830.64900.20990.070*
C140.9214 (5)0.7395 (4)0.1285 (3)0.0693 (14)
H141.00360.69600.11990.083*
C150.9155 (6)0.8333 (5)0.0885 (4)0.0774 (16)
H150.99520.85440.05350.093*
C160.7916 (6)0.8952 (4)0.1004 (3)0.0728 (15)
H160.78650.95870.07380.087*
C170.6748 (5)0.8620 (3)0.1524 (3)0.0542 (11)
C180.5314 (6)0.9189 (4)0.1641 (3)0.0569 (12)
C190.4988 (7)1.0115 (4)0.1263 (4)0.0773 (15)
H190.57321.04620.09520.093*
C200.3571 (8)1.0516 (4)0.1350 (4)0.0898 (19)
H200.33371.11370.10930.108*
C210.2488 (7)1.0009 (4)0.1815 (4)0.0795 (16)
H210.15111.02740.18760.095*
C220.2873 (6)0.9105 (4)0.2190 (3)0.0648 (13)
H220.21360.87620.25090.078*
C230.7172 (6)0.8688 (4)0.4065 (4)0.0714 (15)
H230.78560.87010.36040.086*
C240.7644 (8)0.9151 (4)0.4922 (4)0.0890 (19)
H240.86460.94530.50430.107*
C250.6636 (9)0.9163 (4)0.5590 (4)0.094 (2)
H250.69560.94600.61740.113*
C260.5146 (8)0.8738 (4)0.5405 (4)0.0770 (16)
C270.4728 (6)0.8254 (3)0.4541 (3)0.0608 (12)
C280.3210 (6)0.7716 (4)0.4288 (3)0.0583 (12)
C290.2002 (7)0.7733 (5)0.4858 (3)0.0769 (15)
C300.0683 (7)0.7110 (6)0.4585 (4)0.097 (2)
H30−0.01480.71060.49550.117*
C310.0578 (6)0.6485 (6)0.3763 (4)0.0895 (19)
H31−0.02900.60360.35900.107*
C320.1799 (5)0.6552 (4)0.3212 (3)0.0672 (14)
H320.17230.61590.26490.081*
C33−0.0389 (7)0.1281 (5)0.2908 (4)0.0803 (16)
C340.1324 (6)0.3201 (5)0.3430 (3)0.0757 (16)
C35−0.0071 (6)0.4050 (4)0.1912 (3)0.0647 (13)
C36−0.1464 (6)0.2057 (4)0.1273 (3)0.0614 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.05534 (12)0.05933 (13)0.04656 (12)0.00178 (8)0.00450 (8)0.00274 (8)
Ru10.0478 (2)0.0466 (2)0.03638 (18)−0.00686 (15)−0.00820 (15)0.00191 (15)
N10.048 (2)0.047 (2)0.045 (2)−0.0085 (16)−0.0064 (16)0.0112 (17)
N20.049 (2)0.059 (2)0.0334 (19)−0.0091 (17)−0.0069 (15)0.0017 (17)
N30.045 (2)0.056 (2)0.043 (2)−0.0089 (17)−0.0029 (16)0.0033 (17)
N40.060 (2)0.048 (2)0.041 (2)−0.0079 (18)−0.0097 (17)0.0010 (17)
N50.075 (3)0.048 (2)0.047 (2)−0.0064 (19)−0.022 (2)0.0015 (18)
N60.053 (2)0.059 (2)0.043 (2)0.0014 (18)−0.0001 (16)0.0090 (17)
N70.158 (6)0.094 (4)0.102 (4)−0.027 (4)−0.016 (4)0.036 (4)
N80.106 (4)0.159 (6)0.058 (3)−0.032 (4)−0.018 (3)0.014 (3)
N90.119 (4)0.065 (3)0.094 (4)−0.019 (3)−0.038 (3)0.006 (3)
N100.101 (3)0.064 (3)0.069 (3)−0.019 (2)−0.011 (3)0.006 (2)
C10.061 (3)0.065 (3)0.047 (3)−0.009 (2)−0.015 (2)0.012 (2)
C20.081 (4)0.076 (4)0.070 (3)−0.003 (3)−0.018 (3)0.028 (3)
C30.102 (4)0.052 (3)0.085 (4)0.006 (3)−0.007 (3)0.021 (3)
C40.083 (3)0.053 (3)0.068 (3)−0.005 (3)−0.001 (3)0.010 (3)
C5A0.117 (6)0.038 (4)0.073 (5)0.004 (4)−0.005 (4)0.001 (3)
C5B0.137 (14)0.059 (11)0.054 (10)0.042 (10)0.014 (11)−0.003 (9)
C6A0.132 (7)0.043 (4)0.071 (5)−0.017 (4)0.001 (5)−0.015 (4)
C6B0.146 (13)0.087 (12)0.064 (11)0.051 (11)0.045 (11)0.017 (10)
C70.089 (4)0.055 (3)0.061 (3)−0.013 (3)−0.004 (3)−0.003 (3)
C80.107 (4)0.077 (4)0.054 (3)−0.018 (3)−0.016 (3)−0.018 (3)
C90.086 (4)0.085 (4)0.043 (3)−0.011 (3)−0.021 (3)−0.007 (3)
C100.060 (3)0.063 (3)0.041 (3)−0.004 (2)−0.009 (2)0.001 (2)
C110.049 (2)0.053 (3)0.046 (2)−0.010 (2)−0.0026 (19)0.004 (2)
C120.056 (3)0.045 (3)0.051 (3)−0.010 (2)0.002 (2)0.006 (2)
C130.057 (3)0.059 (3)0.057 (3)−0.005 (2)−0.007 (2)0.002 (2)
C140.057 (3)0.085 (4)0.063 (3)−0.009 (3)0.002 (2)−0.005 (3)
C150.070 (4)0.098 (5)0.062 (3)−0.024 (3)0.008 (3)0.004 (3)
C160.075 (4)0.078 (4)0.064 (3)−0.020 (3)−0.004 (3)0.018 (3)
C170.068 (3)0.049 (3)0.041 (2)−0.020 (2)−0.009 (2)0.005 (2)
C180.070 (3)0.044 (3)0.053 (3)−0.007 (2)−0.014 (2)0.002 (2)
C190.093 (4)0.054 (3)0.082 (4)−0.015 (3)−0.012 (3)0.017 (3)
C200.114 (5)0.047 (3)0.104 (5)0.011 (3)−0.031 (4)0.012 (3)
C210.089 (4)0.058 (4)0.089 (4)0.018 (3)−0.015 (3)−0.002 (3)
C220.065 (3)0.067 (3)0.060 (3)0.014 (3)−0.008 (2)−0.004 (2)
C230.080 (4)0.057 (3)0.070 (3)−0.013 (3)−0.023 (3)−0.006 (3)
C240.113 (5)0.058 (4)0.084 (4)−0.014 (3)−0.050 (4)−0.006 (3)
C250.157 (7)0.063 (4)0.055 (4)0.002 (4)−0.029 (4)−0.009 (3)
C260.122 (5)0.057 (3)0.048 (3)0.014 (3)−0.010 (3)−0.006 (3)
C270.094 (4)0.047 (3)0.041 (3)0.013 (2)−0.006 (3)0.006 (2)
C280.077 (3)0.058 (3)0.041 (3)0.017 (2)−0.003 (2)0.008 (2)
C290.095 (4)0.089 (4)0.051 (3)0.026 (3)0.015 (3)0.016 (3)
C300.093 (5)0.143 (6)0.068 (4)0.035 (4)0.031 (3)0.042 (4)
C310.059 (3)0.136 (6)0.079 (4)0.000 (3)0.010 (3)0.045 (4)
C320.054 (3)0.094 (4)0.053 (3)−0.006 (3)0.000 (2)0.015 (3)
C330.098 (4)0.081 (4)0.060 (3)−0.006 (3)0.003 (3)0.007 (3)
C340.068 (3)0.108 (5)0.049 (3)−0.011 (3)−0.002 (3)0.012 (3)
C350.072 (3)0.056 (3)0.061 (3)−0.012 (3)−0.016 (3)0.002 (3)
C360.069 (3)0.052 (3)0.062 (3)−0.004 (2)−0.001 (3)0.006 (2)
Geometric parameters (Å, º) top
Pt1—C331.959 (6)C14—C151.379 (7)
Pt1—C342.000 (5)C15—C161.372 (7)
Pt1—C351.988 (6)C16—C171.379 (6)
Pt1—C361.983 (5)C17—C181.477 (7)
Ru1—N12.068 (3)C18—C191.379 (7)
Ru1—N22.057 (3)C19—C201.357 (8)
Ru1—N32.062 (3)C20—C211.366 (8)
Ru1—N42.049 (4)C21—C221.364 (7)
Ru1—N52.061 (3)C23—C241.375 (7)
Ru1—N62.052 (3)C24—C251.356 (8)
N1—C11.337 (5)C25—C261.372 (8)
N1—C121.372 (5)C26—C271.385 (6)
N2—C101.330 (5)C27—C281.460 (6)
N2—C111.354 (5)C28—C291.383 (7)
N3—C171.345 (5)C29—C301.375 (8)
N3—C131.347 (5)C30—C311.390 (8)
N4—C221.341 (5)C31—C321.377 (7)
N4—C181.360 (6)C1—H10.9300
N5—C231.353 (6)C2—H20.9300
N5—C271.355 (6)C3—H30.9300
N6—C321.343 (5)C5A—H50.9300
N6—C281.360 (5)C5B—H5B0.9300
N7—C331.155 (7)C6A—H60.9300
N8—C341.128 (6)C6B—H6B0.9300
N9—C351.135 (6)C8—H80.9300
N10—C361.153 (6)C9—H90.9300
C1—C21.375 (7)C10—H100.9300
C2—C31.362 (7)C13—H130.9300
C3—C41.390 (7)C14—H140.9300
C4—C5A1.393 (7)C15—H150.9300
C4—C121.397 (6)C16—H160.9300
C5A—C6A1.358 (10)C19—H190.9300
C5B—C261.10 (3)C20—H200.9300
C5B—C6B1.46 (4)C21—H210.9300
C6A—C71.377 (9)C22—H220.9300
C6B—C291.41 (3)C23—H230.9300
C7—C81.388 (7)C24—H240.9300
C7—C111.391 (6)C25—H250.9300
C8—C91.344 (7)C30—H300.9300
C9—C101.389 (6)C31—H310.9300
C11—C121.431 (6)C32—H320.9300
C13—C141.375 (6)
N9···C83.495 (8)C5A···C36i3.676 (9)
N9···C73.611 (8)C8···C7ii3.595 (8)
C3···Pt1i3.888 (6)C9···C6Aii3.597 (10)
C33—Pt1—C3690.0 (2)N2—C10—H10118.9
C36—Pt1—C3590.79 (19)C9—C10—H10118.9
C33—Pt1—C3491.2 (2)N2—C11—C7122.9 (4)
C35—Pt1—C3488.4 (2)N2—C11—C12116.8 (4)
C36—Pt1—C34175.32 (19)C7—C11—C12120.3 (4)
C33—Pt1—C35174.5 (2)N1—C12—C4122.4 (4)
N4—Ru1—N696.40 (14)N1—C12—C11116.1 (4)
N4—Ru1—N295.37 (14)C4—C12—C11121.5 (4)
N6—Ru1—N296.17 (14)N3—C13—C14121.7 (5)
N4—Ru1—N590.28 (14)N3—C13—H13119.1
N6—Ru1—N578.52 (15)C14—C13—H13119.1
N2—Ru1—N5172.67 (14)C13—C14—C15118.8 (5)
N4—Ru1—N378.32 (15)C13—C14—H14120.6
N6—Ru1—N3173.23 (13)C15—C14—H14120.6
N2—Ru1—N388.60 (13)C16—C15—C14119.7 (5)
N5—Ru1—N397.14 (15)C16—C15—H15120.1
N4—Ru1—N1174.48 (13)C14—C15—H15120.1
N6—Ru1—N186.90 (14)C15—C16—C17119.1 (5)
N2—Ru1—N179.84 (14)C15—C16—H16120.5
N5—Ru1—N194.72 (14)C17—C16—H16120.5
N3—Ru1—N198.71 (14)N3—C17—C16121.5 (5)
C1—N1—C12117.9 (4)N3—C17—C18115.1 (4)
C1—N1—Ru1128.7 (3)C16—C17—C18123.3 (5)
C12—N1—Ru1113.2 (3)N4—C18—C19121.4 (5)
C10—N2—C11118.0 (4)N4—C18—C17113.8 (4)
C10—N2—Ru1128.1 (3)C19—C18—C17124.7 (5)
C11—N2—Ru1113.9 (3)C20—C19—C18119.3 (5)
C17—N3—C13119.1 (4)C20—C19—H19120.3
C17—N3—Ru1116.0 (3)C18—C19—H19120.3
C13—N3—Ru1124.8 (3)C19—C20—C21120.1 (5)
C22—N4—C18117.4 (4)C19—C20—H20120.0
C22—N4—Ru1126.1 (3)C21—C20—H20120.0
C18—N4—Ru1116.5 (3)C22—C21—C20118.4 (6)
C23—N5—C27118.3 (4)C22—C21—H21120.8
C23—N5—Ru1126.0 (4)C20—C21—H21120.8
C27—N5—Ru1115.6 (3)N4—C22—C21123.3 (5)
C32—N6—C28118.3 (4)N4—C22—H22118.3
C32—N6—Ru1125.8 (3)C21—C22—H22118.3
C28—N6—Ru1115.9 (3)N5—C23—C24121.6 (6)
N1—C1—C2121.8 (4)N5—C23—H23119.2
N1—C1—H1119.1C24—C23—H23119.2
C2—C1—H1119.1C25—C24—C23119.5 (6)
C3—C2—C1120.9 (5)C25—C24—H24120.3
C3—C2—H2119.6C23—C24—H24120.3
C1—C2—H2119.6C24—C25—C26120.2 (6)
C2—C3—C4119.2 (5)C24—C25—H25119.9
C2—C3—H3120.4C26—C25—H25119.9
C4—C3—H3120.4C5B—C26—C25122.8 (16)
C3—C4—C5A126.1 (5)C5B—C26—C27118.5 (16)
C3—C4—C12117.7 (5)C25—C26—C27118.5 (6)
C5A—C4—C12116.2 (5)N5—C27—C26121.7 (5)
C6A—C5A—C4121.5 (6)N5—C27—C28115.1 (4)
C6A—C5A—H5119.2C26—C27—C28123.2 (5)
C4—C5A—H5119.2N6—C28—C29122.4 (5)
C26—C5B—C6B119 (2)N6—C28—C27114.5 (4)
C26—C5B—H5B120.5C29—C28—C27123.1 (5)
C6B—C5B—H5B120.5C30—C29—C28117.8 (5)
C5A—C6A—C7124.3 (6)C30—C29—C6B139.5 (11)
C5A—C6A—H6117.9C28—C29—C6B101.7 (11)
C7—C6A—H6117.9C29—C30—C31120.8 (5)
C29—C6B—C5B134.1 (19)C29—C30—H30119.6
C29—C6B—H6B113.0C31—C30—H30119.6
C5B—C6B—H6B113.0C32—C31—C30117.9 (6)
C6A—C7—C8126.8 (5)C32—C31—H31121.0
C6A—C7—C11116.2 (5)C30—C31—H31121.0
C8—C7—C11117.0 (5)N6—C32—C31122.6 (5)
C9—C8—C7120.6 (5)N6—C32—H32118.7
C9—C8—H8119.7C31—C32—H32118.7
C7—C8—H8119.7N7—C33—Pt1178.6 (6)
C8—C9—C10119.4 (5)N8—C34—Pt1178.2 (6)
C8—C9—H9120.3N9—C35—Pt1175.2 (6)
C10—C9—H9120.3N10—C36—Pt1176.3 (5)
N2—C10—C9122.2 (5)
C12—N1—C1—C22.6 (7)C22—N4—C18—C17−174.4 (4)
N1—C1—C2—C3−0.5 (8)N3—C17—C18—N4−2.3 (5)
C1—C2—C3—C4−1.6 (8)C16—C17—C18—N4175.1 (4)
C2—C3—C4—C5A−177.5 (6)N3—C17—C18—C19−178.6 (4)
C2—C3—C4—C121.6 (8)C16—C17—C18—C19−1.2 (7)
C3—C4—C5A—C6A177.7 (7)N4—C18—C19—C20−1.9 (7)
C12—C4—C5A—C6A−1.3 (10)C17—C18—C19—C20174.1 (5)
C4—C5A—C6A—C71.7 (13)C18—C19—C20—C210.6 (8)
C26—C5B—C6B—C29−3 (4)C19—C20—C21—C220.4 (9)
C5A—C6A—C7—C8179.6 (7)C18—N4—C22—C21−0.9 (6)
C5A—C6A—C7—C11−1.3 (11)C20—C21—C22—N4−0.3 (8)
C6A—C7—C8—C9−179.3 (7)C27—N5—C23—C243.5 (7)
C11—C7—C8—C91.5 (8)N5—C23—C24—C25−2.0 (8)
C7—C8—C9—C10−0.6 (9)C23—C24—C25—C26−1.5 (9)
C11—N2—C10—C92.5 (6)C6B—C5B—C26—C25−178.5 (14)
C8—C9—C10—N2−1.5 (8)C6B—C5B—C26—C276 (3)
C10—N2—C11—C7−1.4 (6)C24—C25—C26—C5B−172.1 (14)
Ru1—N2—C11—C7178.6 (3)C24—C25—C26—C273.2 (9)
C10—N2—C11—C12178.1 (4)C23—N5—C27—C26−1.7 (7)
C6A—C7—C11—N2−179.8 (5)C23—N5—C27—C28−179.3 (4)
C8—C7—C11—N2−0.5 (7)C5B—C26—C27—N5173.9 (14)
C6A—C7—C11—C120.6 (8)C25—C26—C27—N5−1.7 (8)
C8—C7—C11—C12179.9 (5)C5B—C26—C27—C28−8.7 (15)
C1—N1—C12—C4−2.7 (6)C25—C26—C27—C28175.8 (5)
C1—N1—C12—C11176.4 (4)C32—N6—C28—C29−5.1 (7)
C3—C4—C12—N10.6 (7)C32—N6—C28—C27172.8 (4)
C5A—C4—C12—N1179.7 (5)N5—C27—C28—N66.5 (6)
C3—C4—C12—C11−178.4 (4)C26—C27—C28—N6−171.1 (4)
C5A—C4—C12—C110.7 (7)N5—C27—C28—C29−175.5 (4)
N2—C11—C12—N10.9 (6)C26—C27—C28—C296.8 (7)
C7—C11—C12—N1−179.5 (4)N6—C28—C29—C304.3 (8)
N2—C11—C12—C4180.0 (4)C27—C28—C29—C30−173.4 (5)
C7—C11—C12—C4−0.4 (7)N6—C28—C29—C6B175.2 (10)
C17—N3—C13—C140.0 (6)C27—C28—C29—C6B−2.6 (11)
N3—C13—C14—C151.5 (7)C5B—C6B—C29—C30168.0 (17)
C13—C14—C15—C16−1.4 (7)C5B—C6B—C29—C280 (3)
C14—C15—C16—C17−0.1 (7)C28—C29—C30—C310.0 (9)
C13—N3—C17—C16−1.7 (6)C6B—C29—C30—C31−166.1 (15)
C13—N3—C17—C18175.8 (4)C29—C30—C31—C32−3.3 (9)
C15—C16—C17—N31.7 (7)C28—N6—C32—C311.6 (7)
C15—C16—C17—C18−175.5 (4)C30—C31—C32—N62.5 (8)
C22—N4—C18—C192.0 (6)
Symmetry codes: (i) x+1, y, z; (ii) −x+1, −y+1, −z.

Experimental details

Crystal data
Chemical formula[Ru(C10H8N2)2(C12H8N2)][Pt(CN)4]
Mr892.81
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)8.6251 (10), 12.7842 (15), 14.7039 (17)
α, β, γ (°)94.557 (2), 94.063 (2), 92.637 (2)
V (Å3)1610.0 (3)
Z2
Radiation typeMo Kα
µ (mm−1)4.85
Crystal size (mm)0.38 × 0.22 × 0.2
Data collection
DiffractometerBruker SMART APEX CCD-detector
diffractometer
Absorption correctionGaussian
(XPREP in SAINT; Bruker, 2001)
Tmin, Tmax0.262, 0.512
No. of measured, independent and
observed [I > 2σ(I)] reflections		8622, 5785, 4934
Rint0.037
(sin θ/λ)max (Å−1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.068, 1.00
No. of reflections5785
No. of parameters452
No. of restraints36
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.88, −0.44

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), KENX (Sakai, 2002), SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX and ORTEP (Johnson, 1976).

Selected geometric parameters (Å, º) top
Pt1—C331.959 (6)Ru1—N22.057 (3)
Pt1—C342.000 (5)Ru1—N32.062 (3)
Pt1—C351.988 (6)Ru1—N42.049 (4)
Pt1—C361.983 (5)Ru1—N52.061 (3)
Ru1—N12.068 (3)Ru1—N62.052 (3)
N9···C83.495 (8)C5A···C36i3.676 (9)
N9···C73.611 (8)C8···C7ii3.595 (8)
C3···Pt1i3.888 (6)C9···C6Aii3.597 (10)
C33—Pt1—C3690.0 (2)N4—Ru1—N590.28 (14)
C36—Pt1—C3590.79 (19)N6—Ru1—N578.52 (15)
C33—Pt1—C3491.2 (2)N4—Ru1—N378.32 (15)
C35—Pt1—C3488.4 (2)N2—Ru1—N388.60 (13)
C36—Pt1—C34175.32 (19)N5—Ru1—N397.14 (15)
C33—Pt1—C35174.5 (2)N6—Ru1—N186.90 (14)
N4—Ru1—N696.40 (14)N2—Ru1—N179.84 (14)
N4—Ru1—N295.37 (14)N5—Ru1—N194.72 (14)
N6—Ru1—N296.17 (14)N3—Ru1—N198.71 (14)
Symmetry codes: (i) x+1, y, z; (ii) −x+1, −y+1, −z.
 

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